#------------------------------------------------------------------------------ #$Date: 2009-11-16 02:43:51 +0100 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003393.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003393 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 726 _journal_page_last 729 _publ_section_title ; 1,2-Bis-crown-5-calix[4]arene ; _chemical_formula_moiety 'C44 H52 O10' _chemical_formula_sum 'C44 H52 O10' _chemical_formula_structural 'C44 H52 O10' _chemical_formula_weight 740.89 _space_group_IT_number 13 _symmetry_space_group_name_Hall '-P 2yc' _symmetry_space_group_name_H-M 'P 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y,1/2-z' '-x,-y,-z' 'x,-y,1/2+z' _cell_length_a 18.060(2) _cell_length_b 10.716(1) _cell_length_c 22.338(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.89(2) _cell_angle_gamma 90.00 _cell_volume 3982.7(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.24 _exptl_crystal_density_meas 1.22(2) _exptl_crystal_density_method flotation _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5416 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.00 _cell_measurement_theta_max 45.0 _exptl_absorpt_coefficient_mu 0.67 _cell_measurement_temperature 295 _exptl_crystal_description 'square prism' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 7796 _reflns_number_total 7796 _reflns_number_observed 1851 _reflns_observed_criterion refl_obs_if_I_>_3.0_sigma(I) _diffrn_reflns_av_R_equivalents 0.01 _diffrn_reflns_theta_max 45 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs .11 _refine_ls_wR_factor_obs .11 _refine_ls_wR_factor_all .11 _refine_ls_goodness_of_fit_obs 'XX' _refine_ls_goodness_of_fit_all 'XX' _refine_ls_number_reflns 1851 _refine_ls_number_parameters 325 _refine_ls_hydrogen_treatment 'H atoms not located' _refine_ls_weighting_scheme 'unit' _refine_ls_shift/esd_max .35 _refine_diff_density_max -.25 _refine_diff_density_min .43 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag O International_Tables_Vol_IV_Table_2.2B .047 .003 C International_Tables_Vol_IV_Table_2.2B .000 .001 H International_Tables_Vol_IV_Table_2.2B .000 .000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? ##;MULTAN80 (Main, Fiske, Hull, Lessinger, ## Germain, Declercq & Woolfson, 1980) ##; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv C1 -.1148(8) .0629(13) .3483(7) 6.9(10) C2 -.0387(8) .0169(14) .3599(6) 6.5(10) C3 .0309(8) .0527(12) .4147(6) 6.2(11) C4 .0178(10) .1317(13) .4609(6) 7.4(12) C5 -.0602(10) .1729(14) .4508(7) 8.1(12) C6 -.1269(9) .1428(15) .3932(7) 7.7(12) C7 -.1889(8) .0407(16) .2800(6) 7.9(13) C8 .1134(7) .0187(13) .4174(6) 6.0(10) C9 .1299(6) .1008(13) .3670(6) 5.4(12) C10 .1573(7) .0429(12) .3216(6) 5.7(11) C11 .1652(7) .1126(15) .2706(7) 6.8(12) C12 .1478(7) .2409(14) .2655(7) 6.7(11) C13 .1224(8) .2999(14) .3110(7) 7.3(11) C14 .1117(7) .2279(14) .3601(6) 6.5(11) O15 .1739(5) -.0845(9) .3289(4) 7.1(7) C16 .2582(8) -.1109(16) .3758(8) 9.0(16) C17 .2629(9) -.2511(15) .3852(7) 8.6(12) O18 .2178(5) -.2768(10) .4259(5) 8.6(8) C19 .2220(11) -.4041(16) .4435(9) 10.5(17) C20 .1678(13) -.4272(18) .4787(8) 11.7(18) O21 .0893(11) -.4305(20) .4259(13) 24.0(24) C22 .0374(17) -.4884(29) .4278(12) 20.4(31) C23 -.0433(19) -.4710(19) .3855(17) 20.6(38) O24 -.0719(8) -.3745(17) .3401(8) 17.6(17) C25 -.0575(16) -.2710(34) .3094(14) 26.3(37) C26 -.0012(15) -.2072(20) .3415(10) 15.8(24) O27 -.0308(5) -.0645(9) .3140(4) 6.8(7) C1' -.2973(7) -.3815(14) .3588(7) 6.8(13) C2' -.3631(8) -.4285(13) .3691(6) 6.5(12) C3' -.3925(8) -.3937(13) .4164(6) 6.6(12) C4' -.3370(10) -.3099(17) .4660(7) 9.2(15) C5' -.2670(11) -.2707(16) .4608(8) 10.7(17) C6' -.2444(8) -.2969(15) .4077(7) 8.7(15) C7' -.2821(7) -.4137(16) .2976(6) 7.7(14) C8' -.4724(8) -.4237(14) .4188(6) 7.3(11) C9' -.5343(8) -.3462(13) .3620(6) 5.8(10) C10' -.5985(8) -.4053(12) .3130(6) 5.5(10) C11' -.6530(7) -.3428(14) .2580(6) 6.2(11) C12' -.6428(9) -.2111(14) .2536(7) 7.2(12) C13' -.5795(10) -.1487(13) .3060(7) 7.5(12) C14' -.5240(8) -.2163(13) .3591(7) 6.6(11) O15' -.6073(5) -.5355(9) .3168(4) 6.8(6) C16' -.6585(8) -.5701(14) .3524(7) 7.6(10) C17' -.6488(9) -.7101(15) .3634(7) 7.9(12) O18' -.5675(6) -.7270(9) .4112(5) 7.7(7) C19' -.5527(12) -.8561(17) .4270(9) 11.7(18) C20' -.4614(14) -.8629(22) .4669(9) 14.6(22) O21' -.4438(10) -.8934(15) .4086(9) 18.1(18) C22' -.3603(14) -.9247(24) .4350(10) 15.6(25) C23' -.3478(18) -.9339(21) .3721(15) 19.3(30) O24' -.3391(9) -.8114(20) .3458(7) 18.5(19) C25' -.3935(13) -.7425(27) .3093(9) 17.6(27) C26' -.4222(11) -.6432(15) .3422(7) 10.1(15) O27' -.4131(5) -.5120(9) .3208(3) 6.4(7)